贵铅中铅和金的连续测定

Continuous determination of lead and gold in precious lead

研究建立了贵铅中铅和金的连续测定方法。样品使用硝酸、溴溶解,加入硫酸形成硫酸铅沉淀,与金及杂质元素分离,乙酸-乙酸铵溶解硫酸铅,Na_(2)EDTA滴定铅量;金和不溶渣灰化-碱溶或灰化-王水溶解后火焰原子吸收光谱法测定金量。本方法测定铅的相对标准偏差为0.12%,加标回收率为92.10%96.42%;测定金的相对标准偏差为0.20%0.52%,加标回收率为90.20%97.20%,准确度和精密度良好,符合分析测定要求。

The research established the continuous determination method for lead and gold in precious lead.The samples are dissolved with nitric acid and bromine.Lead sulfate precipitation is generated by adding sulfuric acid,sepa-rating lead from gold and impurities.Acetic acid-ammonium acetate dissolves lead sulfate.And lead content is determined by Na_(2)EDTA titration;gold content is determined by flame atomic absorption spectrometry after ashing-alkali dissolution or ashing-aqua regia dissolution.When lead content is determined,the method has a RSD of 0.12%,the recovery rate of reference materials 92.10%-96.42%;when gold content is determined,the RSD is 0.20%-0.52%,the recovery rate of reference materials is 90.20%-97.20%.The method has good accuracy and precision and is consistent with the requirement of analysis and determination.